CN1408257A - Method for separating and extracting date cyclic nucleotide syrup, dietary fiber and date wax - Google Patents
Method for separating and extracting date cyclic nucleotide syrup, dietary fiber and date wax Download PDFInfo
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- CN1408257A CN1408257A CN02130757A CN02130757A CN1408257A CN 1408257 A CN1408257 A CN 1408257A CN 02130757 A CN02130757 A CN 02130757A CN 02130757 A CN02130757 A CN 02130757A CN 1408257 A CN1408257 A CN 1408257A
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- jujube
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 11
- 235000020357 syrup Nutrition 0.000 title claims abstract description 10
- 239000006188 syrup Substances 0.000 title claims abstract description 10
- 235000013325 dietary fiber Nutrition 0.000 title abstract description 5
- 241001247821 Ziziphus Species 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000001913 cellulose Substances 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- -1 cyclic monophosphate Chemical class 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 235000005911 diet Nutrition 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 235000013305 food Nutrition 0.000 claims description 4
- 150000004676 glycans Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001282 polysaccharide Polymers 0.000 claims description 4
- 239000005017 polysaccharide Substances 0.000 claims description 4
- 235000019750 Crude protein Nutrition 0.000 claims description 3
- 235000008504 concentrate Nutrition 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000000378 dietary effect Effects 0.000 claims description 3
- 235000012054 meals Nutrition 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 102000009123 Fibrin Human genes 0.000 claims description 2
- 108010073385 Fibrin Proteins 0.000 claims description 2
- BWGVNKXGVNDBDI-UHFFFAOYSA-N Fibrin monomer Chemical compound CNC(=O)CNC(=O)CN BWGVNKXGVNDBDI-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002775 capsule Substances 0.000 claims description 2
- 229950003499 fibrin Drugs 0.000 claims description 2
- 238000005325 percolation Methods 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 240000008866 Ziziphus nummularia Species 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000001704 evaporation Methods 0.000 abstract description 2
- 235000021433 fructose syrup Nutrition 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- 229930013930 alkaloid Natural products 0.000 description 2
- 150000003797 alkaloid derivatives Chemical class 0.000 description 2
- 230000000975 bioactive effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 210000000936 intestine Anatomy 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- WCGUUGGRBIKTOS-GPOJBZKASA-N (3beta)-3-hydroxyurs-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C WCGUUGGRBIKTOS-GPOJBZKASA-N 0.000 description 1
- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 241000050051 Chelone glabra Species 0.000 description 1
- 102000001189 Cyclic Peptides Human genes 0.000 description 1
- 108010069514 Cyclic Peptides Proteins 0.000 description 1
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 description 1
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 description 1
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229940100243 oleanolic acid Drugs 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 229940096998 ursolic acid Drugs 0.000 description 1
- PLSAJKYPRJGMHO-UHFFFAOYSA-N ursolic acid Natural products CC1CCC2(CCC3(C)C(C=CC4C5(C)CCC(O)C(C)(C)C5CCC34C)C2C1C)C(=O)O PLSAJKYPRJGMHO-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a separation and extraction method of jujube cyclic nucleotide syrup, dietary fiber and jujube wax, which comprises the steps of drying, cooling and crushing mature jujube pulp, extracting with ethanol, evaporating alcohol extraction residues to dryness and preparing jujube dietary fiber powder; concentrating the alcoholic extractive solution, recovering ethanol, extracting with organic solvent, and separating to obtain fructus Jujubae wax; concentrating the raffinate to obtain the date cyclic nucleotide syrup. The method of the invention realizes the purpose of developing various products according to the active ingredients and the physical and chemical properties of the jujube, and produces novel functional health dietary fiber and cyclic nucleotide high fructose syrup nourishing products suitable for the old, the weak, the sick, the women and other people.
Description
Technical field
The present invention relates to the extractive technique of the effective constituent of fruit, a kind of method of from jujube, extracting bioactive ingredients of more specifically saying so.
Background technology
Jujube is the Rhamnaceae jujube, contain multiple bioactive ingredients (comprising: cyclic monophosphate, cyclopeptide alkaloid, vegetable polysaccharides, pectin, xitix, ursolic acid, Oleanolic Acid, organic acid and mineral nutrient element etc.) in the fruit, has multiple pharmacological effect, being classified as the dietotherapeutic kind by health ministry, is the distinctive Biological resources of China.The kind of present domestic jujube converted products is a lot, comprising: candied date, date nourishing crystalline substance, jujube tea, jujube paste, jujube wine, date haematochrome etc., but these goods are generally rough-wrought product, it is that whole pulp with jujube are that raw material is implemented, the general separation and Extraction that does not relate to effective constituent, do not accomplish to make the best use of everything, thereby be difficult to guarantee the health-care effect of product yet.
Summary of the invention
The purpose of this invention is to provide a kind of method of from jujube, extracting cyclic monophosphate (cAMP) syrup, food fibre (dietary fiber) and jujube wax, thereby guarantee the health-care effect of product, and the purpose that jujube is now rationally utilized.
Separating and extracting method of the present invention may further comprise the steps:
1. be 0.06-0.098MPa with ripe jujube pulp in vacuum tightness, 60-100 ℃ of following vacuum-drying, pulverize dried jujube pulp cooling back, with ethanol the pure soluble components lixiviate in the jujube powder is come out, alcoholic acid content 60-100% (volume/volume) in solvent during lixiviate, the etoh solvent content of optimizing is 75-95%, perhaps flatten sophisticated dried jujube broken, directly extract with the ethanol circulation, obtain alcohol extract and alcohol extracting residue, described extracting mode comprises percolation, single-stage or multistage pickling process, the continuous countercurrent extraction, circumfluence method (Lv Guiyuan, Wang Yitao compiles, " Chinese medicine new product development ", Beijing, the People's Health Publisher, 1997:289);
2. make the jujube dietary fibrin powder after the alcohol extracting residue solvent evaporated that step (1) obtains, through sieve, compressing tablet or encapsulated, make jujube meals cellulose tablet or capsule, wherein main component is: solubility jujube polysaccharide (40%), Mierocrystalline cellulose (30%), crude protein (18%);
3. step (1) gained alcohol extract concentrates earlier and reclaims ethanol, isolates jujube wax with organic solvent extraction then, is used for refining pharmaceutical cpd triterpenic acid and alkaloid, and described organic solvent comprises ethyl acetate, ether, butanols, amylalcohol, sherwood oil and tool mixture.
4. the raffinate of step (2) is made date cyclic nucleotide syrup with method of enrichment, and cyclic monophosphate content wherein can reach 100 microgram/grams, soluble solid content 65-72% (weight).
The jujube polysaccharide amount adopts the analysis of alcohol precipitation weighting method, cellulosic amount to adopt the analysis of acid elution method in step (2) the jujube food fibre, and crude protein quantity adopts the Kjeldahl determination analysis.
Advantage of the present invention and effect:
(1) the present invention's separation and Extraction from date goes out to have the new type of health function meals jujube Mierocrystalline cellulose of whole intestines fat-reducing effect, this product has overcome the shortcoming of the high sugar of traditional date converted products, high calorie, product has characteristics such as high protein intestines effect low in calories, whole is obvious, and aspects such as toxin expelling, lead discharging, regulating blood fat can be used for losing weight.
(2) the jujube wax that separation and Extraction goes out from jujube wherein contains various active compositions such as triterpenic acid, can be used for the multiple active skull cap components of further separation and Extraction.
(3) from jujube, isolate cyclic nucleotide high fructose syrup excellent tonic product.The health care that can be used for crowds such as old, weak, sick, woman is taken good care of.
In sum, extracting method of the present invention has been realized developing the purpose of multiple product by the activeconstituents of jujube and physicochemical property.
Embodiment
Further specify characteristics of the present invention below by specific embodiment
Embodiment
With Removing Kernel for Date (yield about 85%), oven dry, pulverize after being cooled to room temperature, cross 40 mesh sieves, get 50kg and mix, in the diacolation bucket of packing into, extract with diacolation under the 75% ethanol room temperature with equivalent 75% ethanol, collect vat liquor 200kg, the residue centrifugation goes out residual solvent, dries in vacuum drying oven again, gets the about 10kg of jujube dietary cellulose, pulverize the back and cross 60 mesh sieves, directly the tablet of compacting 1 grammes per square metre is the jujube diet cellulose tablet: extracting solution is merged diatomite filtration, concentrate and reclaim ethanol to 60 liters of cumulative volumes, be cooled to below 25 ℃, divide 2 extractions, combining extraction liquid with 60 liters of ethyl acetate, solvent is reclaimed in evaporation under 0.075Mpa vacuum tightness, gets paste jujube wax 0.4kg; Raffinate is concentrated into 65-70% (weight), gets the about 40kg of big date cyclic nucleotide syrup, and wherein cyclic monophosphate content is about 100 microgram/grams, is the finished product date cyclic nucleotide syrup after the packing sterilization.
Claims (2)
1. the separating and extracting method of a date cyclic nucleotide syrup, food fibre and jujube wax is characterized in that comprising following preparation process:
(1) be 0.06-0.098Mpa, 60-100 ℃ of following vacuum-drying with ripe jujube or wild jujube pulp in vacuum tightness, pulverize dried jujube pulp cooling back, with ethanol the pure soluble components lixiviate in the jujube powder is come out, alcoholic acid content 60-100% (volume/volume) in solvent during lixiviate, perhaps flatten sophisticated dried jujube broken, directly extract with the ethanol circulation, obtain alcohol extract and alcohol extracting residue, described extracting mode comprises percolation, single-stage or multistage pickling process, continuous countercurrent extraction, circumfluence method.
(2) make the jujube dietary fibrin powder after the alcohol extracting residue solvent evaporated that step (1) obtains, through sieve, compressing tablet or encapsulated, make jujube meals cellulose tablet or capsule, wherein main component is: solubility jujube polysaccharide, Mierocrystalline cellulose, crude protein;
(3) step (1) gained is pure that extract concentrates recovery ethanol earlier, isolates jujube wax with organic solvent extraction then, and described organic solvent comprises ethyl acetate, ether, butanols, amylalcohol, sherwood oil and composition thereof.
(4) raffinate of step (2) is made date cyclic nucleotide syrup with method of enrichment, and cyclic monophosphate content wherein can reach 100 microgram/grams, soluble solid content 65-72% (weight).
2. when in accordance with the method for claim 1, it is characterized in that step (1) lixiviate in the solvent alcoholic acid content be 75-95% (volume/volume).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021307571A CN1175758C (en) | 2002-09-25 | 2002-09-25 | Method for separating and extracting cyclic nucleotide syrup, dietary fiber and jujube wax from jujube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021307571A CN1175758C (en) | 2002-09-25 | 2002-09-25 | Method for separating and extracting cyclic nucleotide syrup, dietary fiber and jujube wax from jujube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1408257A true CN1408257A (en) | 2003-04-09 |
| CN1175758C CN1175758C (en) | 2004-11-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021307571A Expired - Fee Related CN1175758C (en) | 2002-09-25 | 2002-09-25 | Method for separating and extracting cyclic nucleotide syrup, dietary fiber and jujube wax from jujube |
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| Country | Link |
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| CN (1) | CN1175758C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009070921A1 (en) * | 2007-11-30 | 2009-06-11 | Chi, Yu-Fen | Antimelancholic medicine prepared with jujube camp materials |
| CN101288468B (en) * | 2008-05-23 | 2011-07-20 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
| RU2456014C2 (en) * | 2007-11-30 | 2012-07-20 | Цзогуан ЧЖАН | ANTIMELANCHOLIC MEDICINE PREPARED WITH JUJUBA cAMP MATERIALS |
| CN102670764A (en) * | 2012-05-07 | 2012-09-19 | 南京中医药大学 | Active parts of wild jujube as well as preparation method and application thereof |
| CN101926452B (en) * | 2009-12-25 | 2012-12-05 | 河北农业大学 | Wild jujube leaf total flavone extract and preparation method thereof |
| CN102875625A (en) * | 2012-10-29 | 2013-01-16 | 北京林业大学 | Extraction method of cyclic adenosine monophosphate (cAMP) with antiallergic activity from Chinese date |
| CN103623080A (en) * | 2013-09-25 | 2014-03-12 | 中恩（天津）医药科技有限公司 | High-content jujube cyclic adenosine monophosphate extract and preparation method thereof |
| CN107259426A (en) * | 2016-04-07 | 2017-10-20 | 河北农业大学 | Method for refining date cyclic adenosine monophosphate syrup |
| CN109651471A (en) * | 2018-12-29 | 2019-04-19 | 河北科技大学 | The extracting method of cyclic adenosine monophosphate and cyclic guanosine monophosphate in jujube fruit |
-
2002
- 2002-09-25 CN CNB021307571A patent/CN1175758C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009070921A1 (en) * | 2007-11-30 | 2009-06-11 | Chi, Yu-Fen | Antimelancholic medicine prepared with jujube camp materials |
| RU2456014C2 (en) * | 2007-11-30 | 2012-07-20 | Цзогуан ЧЖАН | ANTIMELANCHOLIC MEDICINE PREPARED WITH JUJUBA cAMP MATERIALS |
| CN101288468B (en) * | 2008-05-23 | 2011-07-20 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
| CN101926452B (en) * | 2009-12-25 | 2012-12-05 | 河北农业大学 | Wild jujube leaf total flavone extract and preparation method thereof |
| CN102670764A (en) * | 2012-05-07 | 2012-09-19 | 南京中医药大学 | Active parts of wild jujube as well as preparation method and application thereof |
| CN102875625A (en) * | 2012-10-29 | 2013-01-16 | 北京林业大学 | Extraction method of cyclic adenosine monophosphate (cAMP) with antiallergic activity from Chinese date |
| CN102875625B (en) * | 2012-10-29 | 2015-07-08 | 北京林业大学 | Extraction method of cyclic adenosine monophosphate (cAMP) with antiallergic activity from Chinese date |
| CN103623080A (en) * | 2013-09-25 | 2014-03-12 | 中恩（天津）医药科技有限公司 | High-content jujube cyclic adenosine monophosphate extract and preparation method thereof |
| CN103623080B (en) * | 2013-09-25 | 2015-10-21 | 中恩（天津）医药科技有限公司 | High-content jujube cyclic adenosine monophosphate extract and preparation method thereof |
| CN107259426A (en) * | 2016-04-07 | 2017-10-20 | 河北农业大学 | Method for refining date cyclic adenosine monophosphate syrup |
| CN107259426B (en) * | 2016-04-07 | 2021-02-09 | 河北农业大学 | Method for refining date cyclic adenosine monophosphate syrup |
| CN109651471A (en) * | 2018-12-29 | 2019-04-19 | 河北科技大学 | The extracting method of cyclic adenosine monophosphate and cyclic guanosine monophosphate in jujube fruit |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1175758C (en) | 2004-11-17 |
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